ASTM D4698-21

Standard Practice for Total Digestion of Sediment Samples for Chemical Analysis of Various Metals

SIGNIFICANCE AND USE
5.1 The chemical analysis of sediments, collected from such locations as streams, rivers, lakes, and oceans can provide information of environmental significance.  
5.2 These practices can be used with either suspended sediment (material actively transported by water) or bed sediment (material temporarily at rest on the bed of a water body).  
5.3 Standardized practices for digesting sediments, for subsequent chemical analysis, will facilitate inter- and intra-areal comparisons as well as comparison of data generated by different groups. The use of total digestions also eliminates the ambiguities and interpretational difficulties associated with partial digestions and the operational definitions that accompany them.
SCOPE
1.1 This practice covers two procedures for the total digestion of sediments for subsequent determination of metals by such techniques as flame atomic absorption spectrophotometry, graphite-furnace atomic absorption spectrophotometry, atomic emission spectroscopy, etc.  
1.2 This practice is applicable in the subsequent determination of volatile, semivolatile, and nonvolatile metals of sediments.  
1.3 Actual metal quantitation can be accomplished by following the various test methods outlined under other appropriate ASTM standards for the metal(s) of interest. Before selecting either of the digestion techniques outlined in this practice, the user should consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D3976 for any special preparatory considerations.  
1.4 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 15.5.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Oct-2021
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.07 - Sediments, Geomorphology, and Open-Channel Flow

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4698 − 21
Standard Practice for
Total Digestion of Sediment Samples for Chemical Analysis
1
of Various Metals
This standard is issued under the fixed designation D4698; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This practice covers two procedures for the total diges-
D1129 Terminology Relating to Water
tion of sediments for subsequent determination of metals by
D1192 Guide for Equipment for Sampling Water and Steam
suchtechniquesasflameatomicabsorptionspectrophotometry,
3
in Closed Conduits (Withdrawn 2003)
graphite-furnace atomic absorption spectrophotometry, atomic
D1193 Specification for Reagent Water
emission spectroscopy, etc.
D3976 Practice for Preparation of Sediment Samples for
1.2 This practice is applicable in the subsequent determina-
Chemical Analysis
tion of volatile, semivolatile, and nonvolatile metals of sedi-
3. Terminology
ments.
3.1 Definitions:
1.3 Actual metal quantitation can be accomplished by fol-
3.1.1 For definitions of terms used in this standard, refer to
lowing the various test methods outlined under other appropri-
Terminology D1129.
ate ASTM standards for the metal(s) of interest. Before
3.2 Definitions of Terms Specific to This Standard:
selecting either of the digestion techniques outlined in this
3.2.1 partial digestion, n—the dissolution of a sediment
practice, the user should consult the appropriate quantitation
matrix such that quantitation will produce a measurement of
standard(s) for any special analytical considerations, and Prac-
less than 95 % of the constituent present in the sample. In such
tice D3976 for any special preparatory considerations.
cases, recovery is operationally defined by the digestion
1.4 The values stated in inch-pound units are to be regarded
procedure.
as standard. The values given in parentheses are mathematical
3.2.2 total digestion, n—the dissolution of a sediment ma-
conversions to SI units that are provided for information only
trixsuchthatquantitationwillproduceameasurementwhichis
and are not considered standard.
more than 95 % of the constituent present in the sample.
1.5 This standard does not purport to address all of the
4. Summary of Practice
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 Many procedures are available for the total digestion of
priate safety, health, and environmental practices and deter-
sediments prior to metal analysis, but almost all the methods
mine the applicability of regulatory limitations prior to use. fall into one of two main classes: fusion and subsequent
For a specific hazard statement, see 15.5. dissolution of the bead, and wet digestion which directly
dissolves the sample with mineral acids. Each of the classes
1.6 This international standard was developed in accor-
has advantages and disadvantages, as do the individual proce-
dance with internationally recognized principles on standard-
dures which fall under them. The two procedures outlined in
ization established in the Decision on Principles for the
this practice were selected because they are the least restricted,
Development of International Standards, Guides and Recom-
in terms of utility, for dealing with a wide variety of matrices.
mendations issued by the World Trade Organization Technical
Before choosing a particular method, the user should consult
Barriers to Trade (TBT) Committee.
the pertinent literature to determine the utility and applicability
1 2
This practice is under the jurisdiction of ASTM Committee D19 on Water and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
and Open-Channel Flow. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2021. Published January 2022. Originally the ASTM website.
3
approved in 1987. Last previous edition approved in 2013 as D4698 – 92 (2013). The last approved version of this historical standard is referenced on
DOI: 10.1520/D4698-21. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4698 − 21
of either method, pr
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4698 − 92 (Reapproved 2013) D4698 − 21
Standard Practice for
Total Digestion of Sediment Samples for Chemical Analysis
1
of Various Metals
This standard is issued under the fixed designation D4698; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice covers two procedures for the total digestion of sediments for subsequent determination of metals by such
techniques as flame atomic absorption spectrophotometry, graphite-furnace atomic absorption spectrophotometry, atomic emission
spectroscopy, etc.
1.2 This practice is applicable in the subsequent determination of volatile, semivolatile, and nonvolatile metals of sediments.
1.3 Actual metal quantitation can be accomplished by following the various test methods outlined under other appropriate ASTM
standards for the metal(s) of interest. Before selecting either of the digestion techniques outlined in this practice, the user should
consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D3976 for any special
preparatory considerations.
1.4 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only and are not considered standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For a specific hazard statement, see Note 715.5.
1.5 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information
only.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
3
D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits (Withdrawn 2003)
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, and
Open-Channel Flow.
Current edition approved Jan. 1, 2013Nov. 1, 2021. Published January 2013January 2022. Originally approved in 1987. Last previous edition approved in 20072013 as
D4698 – 92 (2007).(2013). DOI: 10.1520/D4698-92R13.10.1520/D4698-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4698 − 21
D1193 Specification for Reagent Water
D3976 Practice for Preparation of Sediment Samples for Chemical Analysis
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this practice, refer to Terminology D1129.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total digestion—partial digestion, n—the dissolution of a sediment matrix such that quantitation will produce a measurement
which is more of less than 95 % of the constituent present in the sample. In such cases, recovery is operationally defined by the
digestion procedure.
3.2.2 partial digestion—total digestion, n—the dissolution of a sediment matrix such that quantitation will produce a measurement
of less which is more than 95 % of the constituent present in the sample. In such cases, recovery is operationally defined by the
digestion procedure.
4. Summary of Practice
4.1 Many procedures are available for the total digestion of sediments prior to metal analysis, but almost all the methods
...